Methanol → 476199-03-8

HRID 2220307노트

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HRID 2220307 반응식
[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([O:13]C)=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1.[OH-].[Na+].CO>O>[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 22171205Methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate

생성물 1

HCID 23568964476199-03-8수율 97%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

A mixture of methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate (67.2 g, 280 mmol), sodium hydroxide (45 g, 1.12 mol), methanol (800 mL) and water (400 mL) were stirred at ambient overnight. The methanol was evaporated and the mixture cooled to 0° C. Acidified with concentrated hydrochloric acid and stirred for 20 mins. The yellow solid was filtered, washing with water (3×100 mL). Dried under vacuum at 45° C. overnight, over phosphorus pentoxide to give the title compound (61.4 g, 97%); δH (300 MHz, d6-DMSO) 8.10 (1H, d, ArH) 7.44 (1H, t, ArH) 7.00 (1H, m, ArH) and 4.02 (3H, s, OCH3).

후처리

  1. customThe methanol was evaporated
  2. stirringAcidified with concentrated hydrochloric acid and stirred for 20 mins
  3. filtrationThe yellow solid was filtered
  4. washwashing with water (3×100 mL)
  5. dry with materialDried under vacuum at 45° C. overnight, over phosphorus pentoxide

출처 및 근거

ORD 기록
ord-641be7131acf4ab9b2456b4687512741
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07417064B2

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